CN101591033A - A kind of preparing calcium carbonate powder - Google Patents
A kind of preparing calcium carbonate powder Download PDFInfo
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- CN101591033A CN101591033A CNA2009100407303A CN200910040730A CN101591033A CN 101591033 A CN101591033 A CN 101591033A CN A2009100407303 A CNA2009100407303 A CN A2009100407303A CN 200910040730 A CN200910040730 A CN 200910040730A CN 101591033 A CN101591033 A CN 101591033A
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Abstract
The invention discloses a kind of preparing calcium carbonate powder, step is: A. adds cleaner in calcium chloride solution, is heated to boiling while stirring and leaves standstill 4 ± 1 hours after 30 ± 5 minutes, treats after solution temperature is reduced to room temperature solution to be filled in the reactor; B. the sodium hydroxide solution that with the mole proportioning is 1.0-1.2 adds in the solution of steps A gained, adds the back circulation that finishes and stirs; C. feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 20-35 ℃ in the carbonization process, is stopped reaction when pH=6-7, filters at last, washs, drying makes calcium carbonate powder.Gained submicron high-performance calcium carbonate superfine powder powder specific surface area is 6-9m2/g, narrower particle size distribution, is well suited for applying to high-end MLCC product.
Description
Technical field
The present invention relates to a kind of preparing calcium carbonate powder, relate in particular to the preparation method of the calcium carbonate superfine powder powder of a kind of ceramic condenser MLCC special use.
Background technology
Lime carbonate has characteristics such as production technique is simple, stable performance as a kind of important inorganic chemical product, is widely used in fields such as plastics, rubber, papermaking, coating, daily-use chemical industry.Special quantum size effect, small-size effect, surface effects that it had make it compare with conventional powder body material, all show decided superiority at aspects such as reinforcement, the transparency, dispersiveness, levelling property and thixotropy.Along with the development of the industrial technology of modernization, all trades and professions are more and more higher to the requirement of light calcium carbonate, and demand is also increasing.As produce that the MLCC industry often needs that foreign matter content is low, the special-purpose calcium carbonate superfine powder of high purity, pattern continous-stable, make ultrafine calcium must be towards customizations, become more meticulous, the functionalization direction develops.Though domestic have some producers to have comparatively sophisticated production technique, its main method all is a bubbling style carbonization technique at intermittence, and unslaked lime through digesting the suspension of making 5-15%, is fed carbonic acid gas again and carries out carbonization.The shortcoming of this carborization is: the calcium hydroxide suspension purity that great majority digestion makes is low, the calcium carbonate product foreign matter content height of generation; The solubleness of calcium hydroxide is little, and the bubble size that contains carbonic acid gas is often bigger, because carburizing reagent relates to gas-liquid-solid three-phase system, calcium ion in the solution reacts generation lime carbonate solid at bubble surface and carbonic acid gas, so carbonization speed is slow usually, the big and skewness of the calcium carbonate granule particle diameter that generates, crystal formation also is difficult to control.People are in order to prepare superfine product, usually generate the calcium carbonate superfine powder powder, and in reaction process, control the product patterns by adding additives such as crystal control agent, reaction suppressor, tensio-active agent by control to temperature in the reaction process and carbon dioxide flow.This method can generate the calcium carbonate powder of different-shape according to adding different additives, but also introduces a large amount of impurity simultaneously, is not suitable for the MLCC production field.
Summary of the invention
The technical problem that the present invention need solve provides a kind of specific surface area, even-grained preparing calcium carbonate powder.
The technical problem to be solved in the present invention is achieved through the following technical solutions: a kind of preparing calcium carbonate powder, step is: A, add cleaner in calcium chloride solution, be heated to boiling while stirring and left standstill 4 ± 1 hours after 30 ± 5 minutes, treat after solution temperature is reduced to room temperature solution to be filled in the reactor; B, be that the sodium hydroxide solution of 1.0-1.2 adds in the solution of steps A gained with the mole proportioning; C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 20-35 ℃ in the carbonization process, is stopped reaction when PH=6-7, filters at last, washs, drying makes calcium carbonate powder.
Further: in above-mentioned preparing calcium carbonate powder, the sodium hydroxide solution adding speed of described step B is 67ml ± 5/min, and described circulation churning time is 10 ± 5min.Among the described step C, the carbonic acid gas total flux was controlled at 70-100ml/ minute.Described cleaner is the compound of one or more calcium, as: one or both in calcium oxide, the calcium hydroxide, the weight of these compounds are 1.1-1.8% of calcium chloride weight.In the described reaction kettle body reactive tank is housed, reactive tank is provided with the pore of ventilation body.
Compared with prior art, the present invention has adopted special bubbling style carborization at intermittence, but adopts the new prescription and the technology that are different from traditional digestion method to make presoma, and precursor particle homogeneity, purity are increased substantially.The preparation of presoma calcium hydroxide is starting material with calcium chloride, adopts the compound of one or more calcium, and weight is the 0.1-0.2% of calcium chloride, and purification calcium chloride obtains high-purity calcium chloride.Adding the mole proportioning is the high purity sodium hydroxide solution of 1.3-1.5, and the calcium hydroxide purity height, the size of particles that are generated are even, and pattern is controlled.Under whipped state, highly purified carbonic acid gas is entered in the aqua calcis by the many pores equipment that is evenly distributed in the reactive tank, make the carbonic acid gas uniform distribution that enters in the liquid phase, and bubble diameter is less, CO2 gas and Ca (OH) 2 suspension contacts area increase, have improved CO2 solubleness, have increased [CO3-] ionic concn in the solution.And control Ventilation Rate be 70-100ml/min, the temperature of whole carbonization process is controlled to be 20-40 ℃.Stopped reaction when the pH value of suspension is reduced to 6-7 filters, washing, can obtain the submicron high-performance calcium carbonate superfine powder powder that spherical or near-spherical, even particle size, size-grade distribution are concentrated after 100-120 ℃ of drying.Gained submicron high-performance calcium carbonate superfine powder powder specific surface area is 6-9m2/g, narrower particle size distribution, is well suited for applying to high-end MLCC product.
Description of drawings
Fig. 1 is the SEM figure of the calcium carbonate powder of the embodiment of the invention 1 preparation
Fig. 2 is the SEM figure of the calcium carbonate powder of the embodiment of the invention 2 preparations
Fig. 3 is the SEM figure of the calcium carbonate powder of the embodiment of the invention 3 preparations
Embodiment
Purport of the present invention is that the invention is still intermittently bubbling style carborization, but adopts the new prescription and the technology that are different from traditional digestion method to make presoma, and precursor particle homogeneity, purity are increased substantially.And adopt a kind of special gas-liquid mixed mode to control the carburizing reagent process, and product pattern and particle diameter are control effectively, produce high-performance calcium carbonate superfine powder powder.
At first, the general planning of summary material prescription of the present invention: a kind of preparing calcium carbonate powder, step is: A, add cleaner in calcium chloride solution, be heated to boiling while stirring and left standstill 4 ± 1 hours after 30 ± 5 minutes, treat after solution temperature is reduced to room temperature solution to be filled in the reactor; B, be that the sodium hydroxide solution of 1.0-1.2 adds in the solution of steps A gained, add the back circulation that finishes and stir the mole proportioning; C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 20-35 ℃ in the carbonization process, is stopped reaction when PH=6-7, filters at last, washs, drying makes calcium carbonate powder.
Kind of preparing calcium carbonate powder, step is: A, add the calcium oxide cleaner in calcium chloride solution, its weight is the 0.1-0.2% of calcium chloride weight; Be heated to 80 ± 5 ℃ while stirring, and keep this temperature 20 ± 5min, leave standstill then and be cooled in 50 ℃, solution is filled in the reactor; B, be that the sodium hydroxide solution of 1.3-1.5 adds in the solution of steps A gained, add the back circulation that finishes and stir the mole proportioning; C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 22 ± 2 ℃ in the carbonization process, is stopped reaction when PH=7, filters at last, washs, drying makes calcium carbonate powder.The sodium hydroxide solution adding speed of described step B is 67ml ± 5/min, and described circulation churning time is 10 ± 5min.Among the described step C, the carbonic acid gas total flux was controlled at 75ml/ minute.The weight of described cleaner is 0.1% of calcium chloride weight.In the described reaction kettle body reactive tank is housed, reactive tank is provided with the pore of ventilation body.The calcium carbonate powder of gained is even, and its SEM figure as shown in Figure 1.
Kind of preparing calcium carbonate powder, step is: A, add the calcium hydroxide cleaner in calcium chloride solution, its weight is the 0.1-0.2% of calcium chloride weight; Be heated to 80 ± 5 ℃ while stirring, and keep this temperature 20 ± 5min, leave standstill then and be cooled in 50 ℃, solution is filled in the reactor; B, be that the sodium hydroxide solution of 1.3-1.5 adds in the solution of steps A gained, add the back circulation that finishes and stir the mole proportioning; C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 30 ± 2 ℃ in the carbonization process, is stopped reaction when PH=7, filters at last, washs, drying makes calcium carbonate powder.The sodium hydroxide solution adding speed of described step B is 67ml ± 5/min, and described circulation churning time is 10 ± 5min.Among the described step C, the carbonic acid gas total flux was controlled at 85ml/ minute.The weight that described cleaner is is 0.2% of calcium chloride weight.In the described reaction kettle body reactive tank is housed, reactive tank is provided with the pore of ventilation body.The calcium carbonate powder of gained is even, and its SEM figure as shown in Figure 2.
Embodiment 3
Kind of preparing calcium carbonate powder, step is: A, add calcium oxide, calcium hydroxide cleaner in calcium chloride solution, its weight is the 0.1-0.2% of calcium chloride weight; Be heated to 80 ± 5 ℃ while stirring, and keep this temperature 20 ± 5min, leave standstill then and be cooled in 50 ℃, solution is filled in the reactor; B, be that the sodium hydroxide solution of 1.3-1.5 adds in the solution of steps A gained, add the back circulation that finishes and stir the mole proportioning; C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 38 ± 2 ℃ in the carbonization process, is stopped reaction when PH=7, filters at last, washs, drying makes calcium carbonate powder.The sodium hydroxide solution adding speed of described step B is 67ml ± 5/min, and described circulation churning time is 10 ± 5min.Among the described step C, the carbonic acid gas total flux was controlled at 92ml/ minute.The weight of described cleaner is 0.15% of calcium chloride weight.In the described reaction kettle body reactive tank is housed, reactive tank is provided with the pore of ventilation body.The calcium carbonate powder of gained is even, and its SEM figure as shown in Figure 3.
Claims (5)
1, a kind of preparing calcium carbonate powder, step is:
A, in calcium chloride solution, add cleaner, be heated to boiling while stirring and left standstill 4 ± 1 hours after 30 ± 5 minutes, treat after solution temperature is reduced to room temperature solution to be filled in the reactor;
B, be that the sodium hydroxide solution of 1.0-1.2 adds in the solution of steps A gained, add the back circulation that finishes and stir the mole proportioning;
C, feed carbonic acid gas in the solution of step B under whipped state, carry out carburizing reagent, control reaction temperature is 20-35 ℃ in the carbonization process, is stopped reaction when PH=6-7, filters at last, washs, drying makes calcium carbonate powder.
2, according to the described preparing calcium carbonate powder of claim 1, it is characterized in that: the sodium hydroxide solution adding speed of described step B is 67ml ± 5/min, and described circulation churning time is 10 ± 5min.
3, according to the described preparing calcium carbonate powder of claim 2, it is characterized in that: among the described step C, the carbonic acid gas total flux was controlled at 70-100ml/ minute.
4, according to the described preparing calcium carbonate powder of claim 3, it is characterized in that: described cleaner is one or both in calcium oxide, the calcium hydroxide, and the weight of these compounds is 0.1-0.2% of calcium chloride weight.
5, according to the described preparing calcium carbonate powder of claim 4, it is characterized in that: in the described reaction kettle body reactive tank is housed, reactive tank is provided with the pore of ventilation body.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730734A (en) * | 2012-06-18 | 2012-10-17 | 佛山市松宝电子功能材料有限公司 | Purification method for calcium carbonate |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
| EP3012223A1 (en) * | 2014-10-24 | 2016-04-27 | Omya International AG | PCC with reduced portlandite content |
| JP6788169B1 (en) * | 2019-11-20 | 2020-11-25 | 健司 反町 | Carbon dioxide fixation method, immobilization carbon dioxide production method, and immobilization carbon dioxide production equipment |
| JP6830564B1 (en) * | 2019-11-20 | 2021-02-17 | 健司 反町 | Carbon dioxide fixation method, carbon dioxide production method, and carbon dioxide fixation device |
| CN113912099A (en) * | 2021-11-23 | 2022-01-11 | 新乡学院 | Multilayer calcium carbonate hollow microsphere for drug loading and preparation method and application thereof |
| US11305228B2 (en) | 2019-08-29 | 2022-04-19 | Kenji SORIMACHI | Method for fixing carbon dioxide, method for producing fixed carbon dioxide, and fixed carbon dioxide production apparatus |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100509632C (en) * | 2007-06-27 | 2009-07-08 | 仙桃市中星电子材料有限公司 | Production of high-purity spherical nano-calcium carbonate |
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2009
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730734A (en) * | 2012-06-18 | 2012-10-17 | 佛山市松宝电子功能材料有限公司 | Purification method for calcium carbonate |
| CN102730734B (en) * | 2012-06-18 | 2015-05-20 | 佛山市松宝电子功能材料有限公司 | Purification method for calcium carbonate |
| CN103073039A (en) * | 2013-03-01 | 2013-05-01 | 兰州理工大学 | Method for preparing superfine carbonate powder material |
| US10294115B2 (en) | 2014-10-24 | 2019-05-21 | Omya International Ag | PCC with reduced portlandite content |
| US11021374B2 (en) | 2014-10-24 | 2021-06-01 | Omya International Ag | PCC with reduced portlandite content |
| TWI580639B (en) * | 2014-10-24 | 2017-05-01 | Omya Int Ag | Pcc with reduced portlandite content |
| CN107074577A (en) * | 2014-10-24 | 2017-08-18 | 欧米亚国际集团 | The PCC of portlandite content with reduction |
| JP2017538647A (en) * | 2014-10-24 | 2017-12-28 | オムヤ インターナショナル アーゲー | PCC with reduced portlandite content |
| EP3012223A1 (en) * | 2014-10-24 | 2016-04-27 | Omya International AG | PCC with reduced portlandite content |
| CN107074577B (en) * | 2014-10-24 | 2019-12-06 | 欧米亚国际集团 | PCC with reduced portlandite content |
| WO2016062682A1 (en) * | 2014-10-24 | 2016-04-28 | Omya International Ag | Pcc with reduced portlandite content |
| US11305228B2 (en) | 2019-08-29 | 2022-04-19 | Kenji SORIMACHI | Method for fixing carbon dioxide, method for producing fixed carbon dioxide, and fixed carbon dioxide production apparatus |
| JP6788169B1 (en) * | 2019-11-20 | 2020-11-25 | 健司 反町 | Carbon dioxide fixation method, immobilization carbon dioxide production method, and immobilization carbon dioxide production equipment |
| WO2021100135A1 (en) * | 2019-11-20 | 2021-05-27 | 健司 反町 | Method for fixing carbon dioxide, method for producing fixed carbon dioxide, and device for producing fixed carbon dioxide |
| WO2021100239A1 (en) * | 2019-11-20 | 2021-05-27 | 健司 反町 | Method for fixing carbon dioxide, method for producing fixed carbon dioxide, and device for fixing carbon dioxide |
| JP6830564B1 (en) * | 2019-11-20 | 2021-02-17 | 健司 反町 | Carbon dioxide fixation method, carbon dioxide production method, and carbon dioxide fixation device |
| CN113912099A (en) * | 2021-11-23 | 2022-01-11 | 新乡学院 | Multilayer calcium carbonate hollow microsphere for drug loading and preparation method and application thereof |
| CN113912099B (en) * | 2021-11-23 | 2023-07-07 | 新乡学院 | Medicinal multi-layer calcium carbonate hollow microsphere and preparation method and application thereof |
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| CN101591033B (en) | 2012-10-03 |
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